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摘要
A sensitive and reliable ion-pair reversed-phase high-performance liquid chromatographic (RP-HPLC) method has been developed and validated for the simultaneous determination of D,L-alpha-hydroxymethionine calcium (HMACa), D,L-alpha-ketoisoleucine calcium (KILCa), alpha-ketovaline calcium (KVCa), alpha-ketoleucine calcium (KLCa) and alpha-ketophenylalanine calcium (KPACa) in the compound alpha-ketoacid tablets using tetrabutylammonium hydroxide as an ion-pair reagent. The analytes were separated on a C-18 column (250 mm x 4.6 mm, 5 mu m) with the mobile phase of methanol-potassium dihydrogen phosphate buffer (pH 3.0; 50 mM) (37:63, v/v) at a flow rate of 0.6 mL min(-1). The UV detection wavelength was set at 210 nm. Good linearity with correlation coefficients larger than 0.9990 (n=6) for all analytes were achieved. The average recoveries were within the range of 99.6-100.9%, and the RSDs of the results were within the acceptable limit of 2.0%, which showed that this method was accurate and precise. The limits of detection were 10.44, 5.94, 3.44, 3.60 and 1.63 ng mL(-1), and the limits of quantification were 34.80, 19.80, 10.32, 12.00 and 5.44 ng mL(-1) for HMACa, KILCa, KVCa, KLCa and KPACa, respectively. The method is simple and accurate for quality control of the compound a-ketoacid tablets.
- 出版日期2012-7
- 单位沈阳药科大学
